Richard escales and milano novak



UNITED STATES rnrnnrr OFFICE.

MANUFACTURE OF EXPLOSIVES.

Specification of Letters Patent.

Patented March 16, 1909.

. Application filed October 16, 1907. Serial No. 397,722.

To all whom it may concern:

Be it known that we, RICHARD ESCALES and M ILANO NOVAK, citizens of Germany and Austria-Hungary; respectively, residing at Munich, Bavaria, Germany, have invented certain new and useful Improvements in'the Manufacture of Explosives; and we do hereby declare the followin to be a full, clear, and exact'description of t e invention, such as will enable others skilled in the art to which it appertains to make and use the same.

In order to reduce the freezing point of nitro-glycerin and of the explosives manufactured from the same, it has been customary to add to the former various admixtures, such as nitrobenzol, dinitroglycerin, nitrated chlorhydrin etc, which can in many cases be manufactured together with the nitroglycerin.

The present invention relates to the manufacture of explosiveshaving. a low freezing.

point and containing nitroglycerin from material obtained according to a process which may be considered as a modification of the Lourenzo method (see Liebigs Annalee, Vol. 119, page 228) for the isolation of glycerin or po yglycerin condensed with hydro- ,chloric acid. This process consists in'mixing one part of glycerin with about to part b weight of water or of a watery solution 0 hydrochloric acid not exceeding of the weight of glycerin present, whereupon a stream of hydrochloric acid is passed through the liquid for several hours at a temperature of about 100 centigrade; to the nnxture is then added an equal quantity of lycerin and the product thus obtained is en jected to a temperature of about 110 centigrade for about 20 to 24 hours. This heating serves to produce a number of condensation products of glycerin and of glycerin with hydrochloric acid. Heating 1s convenientl performed under an ordinary reflux condenser. Instead of diluting strong glycerin or what is known as d namite glycerine (s ecific gravity 1.262) with water, it is also possible to use di uted glycerin alreadycontaining the desired quantity of water. addin an approximately equal ua'ntity of lycerm to the diluted glycerin l iefore conensati'on and after .the stream of hydro chloric acid has been passed through under.

a temperature of about 100, it is permissible to ad smaller quantities of glycerin or the .spondingly varying freezing point.

Also, instead of condensation can be immediately undertaken without further addition of glycerin. After condensation any remaining free hydrochloric acid, which might be harmful during the following nitrating of the products of condensation, may be expelled by heating-to- 150 or 160 centigrade, It is also posslble to saturate the ordinary dynamite glycerin of specific gravity 1.262without any dilutionwitl1 gaseous hydrochloric acid during several hours or to the desired point of saturation and then condense at about 150 centigrade.

During the condensation of the glycerin, with itself and with the hydrochloric acid a product is formed, containing besides unalteied glycerin, the following substances: (1.) monochlorhydrin, (2.) dichlorhydrin, (3.) diglycerin, (4.) chlorhydrin of diglyccrin, (5. rtriglycerin, (6.) chlorhydrin of triglycerin. This mixture is now'subjected to the ordinary process of nitration, during which, besides the trinitroglycerin, also the nitrates of 't-he above-mentioned coin ositions are formed, of which more especia ly the various nitrochlorhydrins cause the mixture to assume a low freezing point. According to the longer or shorter time that the stream of hydrochloric acid acts upon the glycerin, and according to the duration of the condensation, it is possible to obtain, after the subsequent nitration, explosives (Intro-glycerin) of a corre Any of t we ordinary processes of nitration maybe em ployed in converting the product so obtained into a no1i-freezing Intro-explosive. 1* or instance such product may be nitrate-d at a low temperature by the action of a mixture of nitric and sulfuric acids, using one of strong nitric acid and two parts 0 sulfuric acid for every one part of such product, said productbeing gradually addcdio the acidmixture under constant stirring, and the nitrated product finally washed well with cold water.

What we claim as our invention and'desire to secure by Letters Patent, is

1. The process of prod'ucin a nitro-explosive of low freezing point, w ich consists in nitrating a mixture of glycerin witlt 01yglycerins and chlorhydrin compoun, s of monolycerin and oly lycerins.

2. file process 0 producing a nitro-explo- 'sive compound of low freezing point, which strong consists in submittin lycerin to the action i [n testimon whereof we hereunto affix our of water and hydroc lfiaric acid at substansignatures in t 1e presence of two witnesses. 10 tially 100 centigrade, a ding to the product thus obtained a substantially equal quantity of glycerin and heating to substantially 110 I oent grade, removing the remainder of free Witnesses:

hydrochlorie acid and then nitrating the re- 5 LOUIS I. MUELLER, sultant condensation product. 1 ABRAHAM SCHLESINGER. 

